CN113125493B - Instrument for analyzing maleic anhydride crystallization point - Google Patents
Instrument for analyzing maleic anhydride crystallization point Download PDFInfo
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- CN113125493B CN113125493B CN202110403720.2A CN202110403720A CN113125493B CN 113125493 B CN113125493 B CN 113125493B CN 202110403720 A CN202110403720 A CN 202110403720A CN 113125493 B CN113125493 B CN 113125493B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
- G01N25/147—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation by cristallisation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
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Abstract
The invention discloses an instrument for analyzing maleic anhydride crystallization points, and belongs to the technical field of petrochemical industry detection equipment. The utility model provides an instrument of analysis maleic anhydride crystallization point, includes the crystallization pipe, the top of crystallization pipe is provided with the sealing plug, the inside of crystallization pipe is provided with temperature sensing, the inside of crystallization pipe is provided with agitating unit, the outside of crystallization pipe is provided with drive arrangement, agitating unit pierces the sealing plug is connected to drive arrangement, the outside of crystallization pipe is provided with photosensitive device, the outside of crystallization pipe is provided with controls the display stand. According to the invention, automatic numerical value acquisition and threshold value perception are realized, the change points do not need to be manually determined, the photosensitive analysis and the temperature change analysis are matched, and a plurality of curves are comprehensively matched and analyzed, so that the high sensitivity and the high accuracy are realized, and the reliability of the data is improved; the method can be widely applied to sample analysis work in various states and types, and solid and liquid do not need to be distinguished.
Description
Technical Field
The invention relates to the technical field of petrochemical industry detection equipment, in particular to an instrument for analyzing maleic anhydride crystallization points.
Background
The crystallization point refers to a constant temperature or a rising maximum temperature measured in a liquid phase when crystallization occurs by cooling a liquid sample under a specified condition, and is generally expressed by the temperature, and is one of the physical properties of chemical products. For the sample with supercooling phenomenon, the temperature is reduced to be lower than the crystallization temperature at the beginning, then the temperature is naturally raised rapidly to reach a certain maximum temperature, and after the temperature stays for a period of time, the temperature is reduced again, and the maximum temperature is the crystallization point; for the sample without supercooling, the temperature is constant and does not rise any more in a certain period of time in the temperature falling process, and then falls again, and the constant temperature is the crystallization point.
Industrial maleic anhydride is combustible, toxic, corrosive and irritant, and can cause burn of human body; dust and steam are irritating, and can cause pharyngitis, laryngitis and bronchitis after inhalation, and can be accompanied with abdominal pain; the direct contact of eyes and skin has obvious stimulation effect and causes burn; sensitization, can cause rash and asthma; chronic effects, chronic conjunctivitis, nasal mucosal ulcers and inflammation.
In GBT7533-1993, method for measuring crystallization Point of organic chemical product, a thermometer detection mode is adopted for sample analysis. The contact between operators and chemical products is more, and potential hazard influence exists; meanwhile, the solid and liquid products need to be analyzed in different modes, and the steps are complicated; moreover, a manual observation method is adopted, and the timeliness and the instability exist; moreover, the sampling data are few, the type is single, the precision is low, and the final result has deviation.
Disclosure of Invention
The invention aims to provide an instrument for analyzing maleic anhydride crystallization points, which has the advantages of wide application range, convenient operation, intelligence, less manual operation and high accuracy, and solves the problems in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides an instrument of analysis maleic anhydride crystallization point, includes the crystallization tube, the top of crystallization tube is provided with the sealing plug, the inside of crystallization tube is provided with temperature sensing, the inside of crystallization tube is provided with agitating unit, the outside of crystallization tube is provided with drive arrangement, agitating unit pierces the sealing plug is connected to drive arrangement, the outside of crystallization tube is provided with photosensitive device, the outside of crystallization tube is provided with controls the display table, temperature sensing, drive arrangement and photosensitive device are connected to control the display table, photosensitive device comprises light source, reflection sensitization portion and transmission sensitization portion constitute the ring and cup joint the surface of crystallization tube, the light source sets up the central point of reflection sensitization portion surface, the transmission path of light source with the axis of crystallization tube is crossing.
Preferably, the temperature sensors are arranged on the inner wall surface of the crystallization tube, the number of the temperature sensors is a plurality of, and the temperature sensors are arranged at different height positions of the inner wall surface of the crystallization tube.
Preferably, the stirring device comprises a stirring shaft and stirring blades, the stirring blades are arranged on the outer surface of the stirring shaft, the stirring shaft is connected to the driving device, the diameter of the stirring blades is smaller than half of the diameter of the crystallization tube, the stirring shaft is arranged at one side of the upper surface of the sealing plug, and the running track of the stirring blades deviates from the central axis of the crystallization tube.
Preferably, the temperature sensor is arranged on the outer surface of the stirring shaft, the number of the temperature sensors is a plurality of, and the plurality of the temperature sensors are arranged at different height positions of the stirring shaft.
Preferably, an adjusting ring is arranged on the outer surface of the photosensitive device, the photosensitive device is connected with the crystallization tube in a sliding mode, and the photosensitive device is fixed on the outer surface of the crystallization tube through the adjusting ring.
Preferably, the number of the photosensitive devices is a plurality, and the photosensitive devices are sleeved on the outer surface of the crystallization tube.
Preferably, the number of the light sources is three, the three light sources are distributed into three layers from top to bottom, the emitting paths of the light sources on the upper layer are obliquely upwards arranged, the emitting paths of the light sources on the middle layer are horizontally arranged, the emitting paths of the light sources on the lower layer are obliquely downwards arranged, and the emitting paths of the three light sources are all intersected with the central axis of the crystallization tube.
Preferably, a support is arranged outside the crystallization tube, a first support arm is arranged on the support, a first lantern ring is arranged in the middle section of the first support arm, and the crystallization tube is inserted into the first lantern ring.
Preferably, the inner side of the support is provided with a second support arm, the middle section of the second support arm is provided with a second lantern ring, a temperature control container is inserted in the second lantern ring, the outer surface of the temperature control container is provided with a temperature control device, the lower part of the first support arm is provided with a telescopic arm, and the temperature control device and the telescopic arm are connected to the control display table.
A method of analyzing maleic anhydride crystallization point, comprising the steps of:
s1: placing materials, placing a sample to be detected into a crystallization tube, and enabling the temperature state of the sample to be detected to be higher than the temperature of the crystallization state;
s2: the photosensitive device is arranged, the photosensitive device is arranged on the outer surface of the crystallization tube, and a light source is started to control the display table to record the light sensation curves of the reflection photosensitive part and the transmission photosensitive part;
s3: stirring: the temperature sensing and stirring device is arranged in the crystallization tube, submerged temperature sensing is selectively started according to the volume of the material, the display table is controlled to record a temperature curve, and the driving device is started to stir;
s4: curve analysis: stopping stirring when the light sensation curve changes or the temperature curve abnormally rises or stabilizes;
s5: and obtaining a crystallization point value: and obtaining the crystallization point value according to the temperature curve.
Compared with the prior art, the invention provides an instrument for analyzing maleic anhydride crystallization points, which has the following beneficial effects:
1. according to the invention, automatic numerical value acquisition and threshold perception are realized, the change points are not required to be manually determined, the photosensitive analysis and the temperature change analysis are matched, and a plurality of curves are comprehensively matched and analyzed, so that the method has high sensitivity and high accuracy, and the reliability of data is improved.
2. The invention can be widely applied to sample analysis work in various states and types by matching with temperature control adjustment, solid and liquid do not need to be distinguished, the contact between operators and the samples is less, the operation is simple and convenient, and the application range of the equipment is effectively improved.
3. According to the invention, the sealing plug is sealed, so that volatilization generated in the heating or analysis process is avoided, and damage to operators is avoided.
4. According to the invention, a plurality of temperature sensors provide original data support, multi-region temperature data are acquired, integrated and averaged, and the accuracy of the data is improved; the temperature sensing sets up at the (mixing) shaft, reduces the influence of setting up the circuit to the internal environment.
5. According to the invention, the stirring device avoids the emission path of the light source, and fully stirs the sample; the stirring effect of different speeds is realized to drive arrangement variable speed, and early stirring speed is fast, and the later stage is suitably slowed down, reduces the cooling speed of sample to improve data acquisition's precision.
6. According to the invention, the photosensitive devices are sleeved and installed, and are matched and installed according to requirements, so that the convenience of operation is further improved; and the data of samples in different areas are measured through the distribution of a plurality of photosensitive devices, and the analysis of differences improves the analysis accuracy.
7. According to the invention, the three light sources are positioned on the same mounting surface for simultaneous use, and when crystallization is initially generated, multi-angle reflection sensing is performed, so that information change points are obtained more quickly, and the sensitivity to light sense change is improved.
The device has the advantages that the parts which are not involved in the device are the same as or can be realized by adopting the prior art, the automatic value acquisition and threshold sensing are realized, the manual determination of change points is not needed, the photosensitive analysis and the temperature change analysis are matched, and a plurality of curves are comprehensively matched and analyzed, so that the device has high sensitivity and high precision, and the reliability of data is improved; the temperature control adjustment is matched, so that the device can be widely applied to sample analysis work in various states and types, solid and liquid do not need to be distinguished, the contact between operators and the samples is less, the operation is simple and convenient, and the application range of the device is effectively improved; the sealing plug is sealed, so that volatilization generated in the heating or analysis process is avoided, and damage to operators is avoided; the temperature sensors provide original data support, multi-region temperature data are acquired, integrated and averaged, and the accuracy of the data is improved; the temperature sensor is arranged on the stirring shaft, so that the influence of the arrangement circuit on the internal environment is reduced; the stirring device avoids the emission path of the light source and sufficiently stirs the sample; the driving device changes speed to realize stirring effects of different speeds, the early stirring speed is high, the later stirring speed is properly slowed down, and the cooling speed of the sample is reduced so as to improve the accuracy of data acquisition; the photosensitive devices are sleeved and installed, and are matched and installed according to requirements, so that the convenience of operation is further improved; and the data of the samples in different areas are measured through the distribution of a plurality of photosensitive devices, and the analysis accuracy is improved through differential analysis; three light sources are arranged on the same mounting surface and used simultaneously, when crystallization is initially generated, multi-angle reflection sensing is performed, information change points are obtained more quickly, and sensitivity to light sensation change is improved.
Drawings
FIG. 1 is a schematic diagram of a first embodiment;
FIG. 2 is a schematic diagram showing a structure of a crystallization tube according to the first embodiment;
FIG. 3 is a schematic cross-sectional view of a crystallization tube according to the first embodiment;
FIG. 4 is a schematic top sectional view of a crystallization tube according to the first embodiment;
FIG. 5 is a right-side view of a photosensitive device according to the first embodiment;
FIG. 6 is a schematic cross-sectional view of a crystallization tube according to a second embodiment;
FIG. 7 is a schematic diagram showing the structure of a crystallization tube according to the third embodiment;
FIG. 8 is a right-side view schematically illustrating a photosensitive device according to a third embodiment;
fig. 9 is a schematic diagram showing the structure of a fourth heating state of the embodiment;
fig. 10 is a schematic sectional structure diagram of a fourth heating state of the embodiment;
fig. 11 is a schematic structural view of a stirring state of the fourth embodiment.
In the figure: 1. a crystallization tube; 2. a sealing plug; 3. temperature sensing; 4. a stirring device; 401. a stirring shaft; 402. stirring the leaves; 5. a driving device; 6. a photosensitive device; 601. a light source; 602. a reflective photosensitive section; 603. a transmission photosensitive part; 7. an adjusting ring; 8. a bracket; 9. a first arm; 10. a first collar; 11. a second arm; 12. a second collar; 13. a temperature control container; 14. a temperature control device; 15. and a telescopic arm.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In the description of the present invention, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Embodiment one:
referring to fig. 1-5, an apparatus for analyzing maleic anhydride crystallization point includes a crystallization tube 1, wherein the crystallization tube 1 is preferably made of a high-transmittance, high-strength and high-temperature-resistant material to reduce the influence on transmitted light; the top of the crystallization tube 1 is provided with the sealing plug 2, so that the top of the crystallization tube 1 is sealed, and a large amount of volatilization is avoided in the heating or analysis process, and the damage to operators is avoided; the inside of the crystallization tube 1 is provided with a temperature sensor 3 for acquiring temperature data of a sample to be detected in real time and providing an original data support; the inside of the crystallization tube 1 is provided with a stirring device 4, the outside of the crystallization tube 1 is provided with a driving device 5, and the stirring device 4 penetrates through the sealing plug 2 and is connected to the driving device 5 to provide stirring power input for the sample; the outer side of the crystallization tube 1 is provided with a photosensitive device 6, and the photosensitive device 6 consists of a light source 601, a reflection photosensitive part 602 and a transmission photosensitive part 603; the reflective photosensitive part 602 is a half ring, the transmissive photosensitive part 603 is a half ring, and the reflective photosensitive part 602 and the transmissive photosensitive part 603 are combined to form a ring to be sleeved on the outer surface of the crystallization tube 1; the light source 601 is arranged at the center of the outer surface of the reflection photosensitive part 602, the reflection photosensitive part 602 is positioned between the light source 601 and the crystallization tube 1, and a strip-shaped hole is formed for the front end of the light source 601 to penetrate into and reach the outer surface of the crystallization tube 1; the outer surface of the reflective photosensitive part 602 is provided with a rotary bracket, the rotary bracket consists of two vertical plates which are symmetrically arranged, the light source 601 is arranged between the vertical plates, two sides of the light source 601 are rotationally connected with the rotary bracket through a rotating shaft inserted in the vertical plates, and the incident angle of the emitting path of the light source 601 can be adjusted; the emitting path of the light source 601 intersects with the central axis of the crystallization tube 1 and avoids the stirring device 4, so that light is prevented from being blocked; the light source 601 is preferably a high-polymerization, single light source; by utilizing the change of the crystal physical form of the sample, the light transmittance changes during crystallization, the light sensation curve of the transmission photosensitive part 603 changes, and the reflection effect after crystallization is enhanced, and the light sensation curve of the reflection photosensitive part 602 changes; the method can quickly react when crystallization occurs, improves the timeliness of data acquisition and improves the accuracy; the outside of the crystallization tube 1 is provided with a control display table, and the temperature sensing 3, the driving device 5 and the photosensitive device 6 are connected to the control display table, and the control display table controls the control display table and displays a data curve for analysis.
The stirring device 4 consists of a stirring shaft 401 and stirring blades 402; the stirring shaft 401 penetrates the sealing plug 2 to be connected to the driving device 5, the sealing plug 2 is provided with holes for the stirring shaft 401 to pass through, and a wear-resistant pipeline can be arranged in the holes to enhance the durability of the stirring shaft 401 and improve the stability of the stirring shaft 401; stirring leaf 402 sets up the surface at (mixing) shaft 401, and stirring leaf 402's quantity is a plurality of, fully stirs the sample for its cooling rate. The stirring shaft 401 is arranged at one side of the upper surface of the sealing plug 2, the diameter of the stirring blade 402 is smaller than half of the diameter of the crystallization tube 1, and the outer edge of the stirring blade 402 is close to the inner wall of the crystallization tube 1 but is not contacted with the inner wall; the running track of the stirring blade 402 deviates from the central axis of the crystallization tube 1 and does not intersect with the central axis; the whole stirring device 4 runs in a quarter space at one side of the crystallization tube 1 and is not contacted with the tube wall and the central axis of the crystallization tube 1. The driving device 5 is a variable speed motor, so that stirring effects of different speeds are realized, the early stirring speed is high, the later stirring speed is properly slowed down, and the cooling speed of the sample is reduced, so that the accuracy of data acquisition is improved. The temperature sensors 3 are arranged on the outer surface of the stirring shaft 401, the number of the temperature sensors 3 is a plurality, and the temperature sensors 3 are arranged at different height positions of the stirring shaft 401 so as to acquire multi-region temperature data of a sample, integrate and average the multi-region temperature data and improve the accuracy of the data; the temperature sensor 3 is connected to external communication through the stirring shaft 401, reducing the influence of the arrangement line on the internal environment.
The outer surface of the photosensitive device 6 is provided with an adjusting ring 7, the photosensitive device 6 is in sliding connection with the crystallization tube 1, and the photosensitive device 6 is fixed on the outer surface of the crystallization tube 1 through the adjusting ring 7; the structure of the reflection photosensitive part 602 and the transmission photosensitive part 603 divided into two parts can move on the outer surface of the crystallization tube 1 under the condition of not being subjected to external constraint pressure; after the required installation position is determined, the adjusting ring 7 is used for attaching the adjusting ring to the outer surface of the crystallization tube 1 and fixing the crystallization tube; the adjusting ring 7 can be of various types such as a fastening ring or a rubber ring, the fastening ring needs to be locked, and the rubber ring can be locked quickly by utilizing the elasticity of the fastening ring.
The number of the photosensitive devices 6 is a plurality, and the photosensitive devices 6 are uniformly distributed on the outer surface of the crystallization tube 1; a plurality of photosensitive devices 6 are arranged to measure the data of samples in different areas, and differential analysis is performed, so that the accuracy of analysis is improved.
The outside of the crystallization tube 1 is provided with a bracket 8, the bracket 8 is provided with a first support arm 9, the middle section of the first support arm 9 is provided with a first lantern ring 10, and the crystallization tube 1 is inserted into the first lantern ring 10; the inner circumferential surface of the first collar 10 is provided with a rubber layer to improve friction and reduce abrasion of the crystallization tube 1. The driving device 5 is arranged at the upper part of the first support arm 9, and the driving device 5 is detachably connected with the first support arm 9; the driving device 5 and the sealing plug 2 can be connected into a whole through a connecting rod, so that the stability and the installation speed of the sealing plug are improved; and the detachable connection with the first support arm 9 is realized through the forms of inserting connection, bolts and the like; and after the analysis operation is finished, the device is quickly dismantled for cleaning and maintenance. The whole equipment is placed to setting up support 8, improves convenience, the stability of removal and operation.
Embodiment two:
please refer to fig. 6: the difference from the first embodiment is that the temperature sensor 3 is disposed on the inner wall surface of the crystallization tube 1, the shape of the temperature sensor 3 is matched with the inner wall surface of the crystallization tube 1, and the temperature sensor is avoided from the emission path of the light source 601 and the moving track of the stirring device 4; the temperature sensor 3 is preferably a thin and deformable structure so as to be fully attached to the inner wall of the crystallization tube 1 and reduce the influence on the internal environment; the temperature sensor 3 is connected to the outside through a connecting wire which is also attached to the inner wall surface; the number of the temperature sensors 3 is a plurality of, and the temperature sensors 3 are arranged at different height positions of the inner wall surface of the crystallization tube 1.
Embodiment III:
please refer to fig. 7-8: the difference from the first embodiment is that the number of the light sources 601 is three, and the three light sources 601 are distributed into three layers from top to bottom; the emission paths of the upper light source 601 are obliquely upwards, the emission paths of the middle light source 601 are horizontally arranged, the emission paths of the lower light source 601 are obliquely downwards arranged, and the emission paths of the three light sources 601 are all intersected with the central axis of the crystallization tube 1; in the angle adjustment process, it is ensured that the light source reaches the recognition range of the transmission photosensitive portion 603 after being refracted. Three light sources 601 are located on the same installation surface and used simultaneously, when crystallization is generated initially, multi-angle reflection sensing can acquire information change points faster, and sensitivity to light sensation change is improved.
Embodiment four:
please refer to fig. 9-11: the difference with the first embodiment is that the inner side of the bracket 8 is provided with a second support arm 11, the middle section of the second support arm 11 is provided with a second lantern ring 12, and the central axis of the second lantern ring 12 coincides with the central axis of the first lantern ring 10; a temperature control container 13 is inserted into the second sleeve ring 12, the inner diameter of the temperature control container 13 is larger than the outer diameter of the crystallization tube 1, and heat conduction liquid is arranged in the temperature control container 13 to transfer energy to the crystallization tube 1, and the heat conduction liquid is preferably a material with high boiling point and high conduction rate; the outer surface of the temperature control container 13 is provided with a temperature control device 14 for realizing the support of temperature regulation; the lower part of the first support arm 9 is provided with a telescopic arm 15, and the temperature control device 14 and the telescopic arm 15 are connected to a control display table. The temperature control container 13 can adopt a thick test tube or other heat and cold resistant devices, and the temperature control device 14 can adopt the modes of electric control temperature adjustment and the like. By additionally arranging a temperature control device, the heating and dissolving functions are provided for the condition that the sample to be tested is solid or other conditions needing to be heated; and the temperature control device 14 is automatically closed after the proper temperature is reached in the crystallization tube 1 by means of the control display table, the telescopic arm 15 is driven to extend and lift the first support arm 9, the crystallization tube 1 is moved out of the temperature control container 13, and subsequent operation is carried out.
A method of analyzing maleic anhydride crystallization point, comprising the steps of:
s1: placing materials, placing a sample to be detected into a crystallization tube, and enabling the temperature state of the sample to be detected to be higher than the temperature of the crystallization state; for the sample to be heated, the temperature-controlled container 13 of the device can be used for heating, or the sample can be placed into a crystallization tube after external heating.
S2: the photosensitive device is arranged, the photosensitive device is arranged on the outer surface of the crystallization tube, and a light source is started to control the display table to record the light sensation curves of the reflection photosensitive part and the transmission photosensitive part; the number and the positions of the photosensitive devices are set according to the placement height of the sample to be detected, a certain interval is reserved in the installation process, and interference generated between the photosensitive devices is reduced.
S3: stirring: the temperature sensing and stirring device is arranged in the crystallization tube, submerged temperature sensing is selectively started according to the volume of the material, the display table is controlled to record a temperature curve, and the driving device is started to stir; and enabling the temperature sensing submerged in the sample to be detected, and enabling the temperature sensing submerged in the sample to be detected.
S4: curve analysis: stopping stirring when the light sensation curve changes or the temperature curve abnormally rises or stabilizes; in combination with its feature, stirring is stopped when either curve is triggered.
S5: and obtaining a crystallization point value: comprehensively analyzing according to temperature curves generated by a plurality of temperature sensors to obtain a crystallization point value; in the analysis of the data, the upper and lower layer curve data can be selectively discarded, and the average value of the rest data can be obtained.
According to the invention, automatic value acquisition and threshold perception are realized, a change point is not required to be determined manually, the photosensitive analysis and the temperature change analysis are matched, and a plurality of curves are comprehensively matched and analyzed, so that the high sensitivity and the high accuracy are realized, and the reliability of data is improved; the temperature control adjustment is matched, so that the device can be widely applied to sample analysis work in various states and types, solid and liquid do not need to be distinguished, the contact between operators and the samples is less, the operation is simple and convenient, and the application range of the device is effectively improved; the sealing plug 2 is used for sealing, so that volatilization generated in the heating or analysis process is avoided, and the injury to operators is avoided; the temperature sensors 3 provide original data support, acquire multi-region temperature data, integrate and average the multi-region temperature data, and improve the accuracy of the data; the temperature sensor 3 is arranged on the stirring shaft 401, so that the influence of a setting circuit on the internal environment is reduced; the stirring device 4 avoids the emission path of the light source 601 and sufficiently stirs the sample; the driving device 5 realizes stirring effects of different speeds through speed change, the early stirring speed is high, the later stirring speed is properly slowed down, and the cooling speed of the sample is reduced so as to improve the accuracy of data acquisition; the photosensitive devices 6 are sleeved and installed, and are matched and installed according to requirements, so that the convenience of operation is further improved; and the data of the samples in different areas are distributed and measured through a plurality of photosensitive devices 6, and the analysis precision is improved through differential analysis; three light sources 601 are located on the same installation surface and used simultaneously, when crystallization is initially generated, multi-angle reflection sensing is performed, information change points are obtained more quickly, and sensitivity to light sensation change is improved.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. The instrument for analyzing maleic anhydride crystallization points is characterized by comprising a crystallization tube (1), wherein a sealing plug (2) is arranged at the top of the crystallization tube (1), a temperature sensing (3) is arranged in the crystallization tube (1), a stirring device (4) is arranged in the crystallization tube (1), a driving device (5) is arranged outside the crystallization tube (1), the stirring device (4) penetrates through the sealing plug (2) and is connected to the driving device (5), a photosensitive device (6) is arranged outside the crystallization tube (1), a control display table is arranged outside the crystallization tube (1), the temperature sensing (3), the driving device (5) and the photosensitive device (6) are connected to the control display table, the photosensitive device (6) consists of a light source (601), a reflecting photosensitive part (602) and a transmitting photosensitive part (603), a circular ring is sleeved on the outer surface of the crystallization tube (1), the light source (601) is arranged at the position of the reflecting part (602) and is away from the center of the light source (603), and the center line (4) of the light source (1) is intersected with the stirring path (4);
the outer surface of the reflection photosensitive part (602) is provided with a rotary bracket, the rotary bracket consists of two vertical plates which are symmetrically arranged, two sides of the light source (601) are rotationally connected with the rotary bracket through a rotating shaft which is inserted in the vertical plates, and the incident angle of the emitting path of the light source (601) can be adjusted;
the outer surface of the photosensitive device (6) is provided with an adjusting ring (7), the photosensitive device (6) is in sliding connection with the crystallization tube (1), and the photosensitive device (6) is fixed on the outer surface of the crystallization tube (1) through the adjusting ring (7);
the number of the photosensitive devices (6) is a plurality, and the photosensitive devices (6) are sleeved on the outer surface of the crystallization tube (1);
the number of the light sources (601) is three, the three light sources (601) are distributed into three layers from top to bottom, the emission paths of the light sources (601) at the upper layer are obliquely upwards arranged, the emission paths of the light sources (601) at the middle layer are horizontally arranged, the emission paths of the light sources (601) at the lower layer are obliquely downwards arranged, and the emission paths of the three light sources (601) are all intersected with the central axis of the crystallization tube (1);
the crystallization device is characterized in that a support (8) is arranged outside the crystallization tube (1), the support (8) is provided with a first support arm (9), a first lantern ring (10) is arranged in the middle section of the first support arm (9), and the crystallization tube (1) is inserted into the first lantern ring (10);
the inside of support (8) is provided with second support arm (11), the middle section of second support arm (11) is provided with second lantern ring (12), temperature control container (13) have been inserted to second lantern ring (12), the surface of temperature control container (13) is provided with temperature regulating device (14), the lower part of first support arm (9) is provided with flexible arm (15), temperature regulating device (14) and flexible arm (15) are connected to control the display stand.
2. The instrument for analyzing maleic anhydride crystallization point according to claim 1, wherein the temperature sensors (3) are arranged on the inner wall surface of the crystallization tube (1), the number of the temperature sensors (3) is a plurality, and the temperature sensors (3) are arranged at different height positions of the inner wall surface of the crystallization tube (1).
3. An instrument for analyzing maleic anhydride crystallization point according to claim 1, characterized in that the stirring device (4) is composed of a stirring shaft (401) and a stirring blade (402), the stirring blade (402) is arranged on the outer surface of the stirring shaft (401), the stirring shaft (401) is connected to the driving device (5), the diameter of the stirring blade (402) is smaller than half of the diameter of the crystallization tube (1), the stirring shaft (401) is arranged on one side of the upper surface of the sealing plug (2), and the running track of the stirring blade (402) deviates from the central axis of the crystallization tube (1).
4. An apparatus for analyzing maleic anhydride crystallization point according to claim 3, wherein the temperature sensors (3) are disposed on the outer surface of the stirring shaft (401), the number of the temperature sensors (3) is several, and the number of the temperature sensors (3) are disposed at different height positions of the stirring shaft (401).
5. A method of using an apparatus for analyzing maleic anhydride crystallization point according to any one of claims 1 to 4, comprising the steps of:
s1: placing materials, placing a sample to be detected into a crystallization tube, and enabling the temperature state of the sample to be detected to be higher than the temperature of the crystallization state;
s2: the photosensitive device is arranged, the photosensitive device is arranged on the outer surface of the crystallization tube, and a light source is started to control the display table to record the light sensation curves of the reflection photosensitive part and the transmission photosensitive part;
s3: stirring: the temperature sensing and stirring device is arranged in the crystallization tube, submerged temperature sensing is selectively started according to the volume of the material, the display table is controlled to record a temperature curve, and the driving device is started to stir;
s4: curve analysis: stopping stirring when the light sensation curve changes or the temperature curve abnormally rises or stabilizes;
s5: and obtaining a crystallization point value: and obtaining the crystallization point value according to the temperature curve.
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